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38 results about "N-butyl nitrite" patented technology

Butyl nitrite is an alkyl nitrite made from n-butanol. Butyl nitrite is used recreationally as poppers. Synonyms include 1-butyl nitrite and nitrous acid, butyl ester. It can be prepared by reacting nitrous acid (generated in situ by reacting a metal nitrite with a mineral acid) with n-butanol.

Modification method of functionalized MXene, diaphragm preparation method and application

The invention discloses a modification method of functionalized MXene, and a preparation method and application of a diaphragm, and belongs to the technical field of flow batteries, the modification method comprises the following steps: preparing MXene from MAX ceramic powder through a mixed acid etching method; preparing an MXene nanosheet; sequentially adding the dried MXene nanosheet, amino-containing aromatic small organic molecules and a diazonium salt initiator according to a molar ratio of (1-1.5): (7-9.5): (7-9.5), wherein the diazonium salt initiator is tert-butyl nitrite or isoamyl nitrite; carrying out vacuum pumping, and reacting for 8-12 hours at the temperature of 60-80 DEG C, so as to obtain the organic micromolecule covalently grafted functionalized MXene. On the basis of mild diazonium salt reaction, different functional groups can be connected according to application requirements to obtain organic micromolecule covalently grafted functionalized MXene, so that the electrochemical performance of the flow battery diaphragm material is improved.
Owner:CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY

Synthetic method of isoxazole compound under visible light catalysis condition

PendingCN121974865AOrganic chemistryOrganic synthesisN-butyl nitrite
The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazole compound under a visible light catalysis condition. The method comprises the following steps: dissolving a compound 1 in 1, 2-dichloroethane, then adding tert-butyl nitrite, tribromomethane, alkali and a photocatalyst, in an inert gas environment, irradiating with visible light and stirring at room temperature to react, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column purification on a crude product to obtain a product, namely the isoxazole compound. The brand-new method for preparing the isoxazole compound through visible light catalysis is developed, the conditions of high temperature and high pressure in a traditional synthesis method are avoided, energy consumption and environmental pollution are remarkably reduced, and the yield of the isoxazole compound is effectively increased by regulating and controlling reaction conditions and optimizing raw material selection and proportion.
Owner:GUANGDONG UNIV OF PETROCHEMICAL TECH

Preparation method of 4-phenoxyphenylboronic acid

The invention discloses a preparation method of 4-phenoxyphenylboronic acid, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: by taking diphenyl ether as a raw material, reacting with fuming nitric acid under the action of tris (pentafluorophenyl) boron, so as to generate a 4-nitrodiphenyl ether intermediate; generating 4-aminodiphenyl ether from the 4-nitrodiphenyl ether intermediate under the action of tetrahydroxy diboron and a catalyst, and then generating 4-phenoxyphenylboronic acid from the 4-aminodiphenyl ether and excessive tetrahydroxy diboron under the action of tert-butyl nitrite. In the first step of the route, the positioning selectivity of 4-position nitro is increased through specific Lewis acid, in the second step, nitro reduction and boronation are carried out through a continuous one-pot method, and the synthesis method of the compound is enriched.
Owner:安徽英特美科技有限公司

A method for the solution process, synergistic catalytic preparation of post-functionalized polyolefins

PendingCN122127542APolymer sciencePolyolefin
This invention discloses a solution-based synergistic catalytic method for preparing post-functionalized polyolefins, belonging to the field of polymer material modification technology. The method includes the following preparation steps: adding polyolefin, graft monomer, and catalyst to an organic solvent, stirring until homogeneous, and heating to react, thereby obtaining the post-functionalized polyolefin; wherein the catalyst is a combination of a first catalyst and a second catalyst; and the first catalyst is selected from tert-butyl nitrite, and the second catalyst is selected from N-hydroxysuccinimide and / or N-hydroxyphthalimide. This invention utilizes a synergistic catalytic system composed of tert-butyl nitrite and N-hydroxysuccinimide and / or N-hydroxyphthalimide to activate the C-H bonds of polyolefins in an organic solvent via a free radical mechanism, thereby grafting polar functionalized graft monomers onto the main chain of various polyolefins.
Owner:CHAIN WALK NEW MATERIAL TECH (GUANGZHOU) CO LTD

Preparation method of methyl 2, 6-dichloro-4-cyanobenzoate

The invention belongs to the technical field of synthesis of ester compounds, and particularly relates to a preparation method of 2, 6-dichloro-4-cyanobenzoic acid methyl ester, which comprises the following steps: by taking dimethyl 2-aminoterephthalate as a raw material, sequentially carrying out substitution reaction, deamination reaction, hydrolysis reaction, amidation reaction and dehydration reaction to obtain the 2, 6-dichloro-4-cyanobenzoic acid methyl ester. The 2, 6-dichloro-4-cyanobenzoic acid methyl ester is prepared by the method, and the yield reaches 59.28%. The N-chlorosuccinimide is used as a chlorine source to carry out substitution reaction on the 2-amino dimethyl terephthalate, so that the potential safety hazard caused by the traditional chlorination reagent is avoided, and the tert-butyl nitrite used in the deamination reaction avoids the potential safety hazard caused by the use of strong corrosive sulfuric acid; the amidation reaction is completed in one step by adopting a condensing agent, so that the complicated operation caused by firstly preparing acyl chloride and then carrying out condensation reaction is avoided, and therefore, the preparation method has the characteristics of safe preparation process, environment friendliness, simplicity in operation and the like under the condition of ensuring the product yield and purity.
Owner:SHANGHAI TITAN SCI CO LTD

Synthetic method of isoxazoline compound

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazoline compound. The preparation method comprises the following steps: dissolving a compound 1 and ethyl acrylate in dichloroethane, then adding tert-butyl nitrite, alkali and K2S2O8, in an air environment, irradiating with a 35 W blue LED light source and stirring at room temperature for 12 hours, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column chromatography on a crude product to obtain a product, namely the isoxazoline compound. The synthesis method provided by the invention avoids the problem of residue of a traditional metal catalyst, and provides a new normal form for green synthesis of the isoxazoline compound. As a key intermediate, isoxazoline can derive beta-lactam, beta-amino alcohol and other structures, and a new path is provided for complex molecule synthesis.
Owner:GUANGDONG UNIV OF PETROCHEMICAL TECH +1

Aryl alkyl ketoxime derivative as well as preparation method and application thereof

The invention provides an aryl alkyl ketoxime derivative as well as a preparation method and application thereof, and relates to the field of aryl oxime derivatives. The preparation method of the aryl alkyl ketoxime derivative comprises the following steps: by taking potassium formate as an additive, carrying out free radical reaction on a compound I and a compound II under ultraviolet irradiation in the presence of tert-butyl nitrite to obtain the aryl alkyl ketoxime derivative, the compound I is substituted iodobenzene or iodopyridine; the compound II is substituted styrene or thienyl ethylene; wherein a hydrogen atom transfer / single electron transfer relay sequence is utilized to activate a compound I, and tert-butyl nitrite is adopted as a bifunctional reagent, and is used as a hydrogen atom transfer reagent and an oxime source. According to the preparation method of the aryl alkyl ketoxime derivative, pre-functionalization is not needed, a reaction substrate is wide in universality and good in compatibility, reaction conditions are mild, operation is easy and convenient, a target product can be efficiently and rapidly prepared on the premise of high yield, and a new way is provided for oxime synthesis.
Owner:JINING UNIV

Scaled-up synthesis of lomustine under continuous flow conditions

To provide a scaled-up synthesis of lomustine under continuous flow conditions.SOLUTION: The present disclosure provides processes and apparatuses for the scaled-up manufacture of lomustine via continuous flow manufacture. Such continuous flow processes may optionally include the crystallization of lomustine and the apparatuses may optionally include crystallization apparatuses / reactors in either batch or continuous flow design. In one aspect of the disclosure, there is provided a process for making lomustine comprising: treating solutions of 2-chloroethylisocyanate with a solution of cyclohexylamine with continuous-flow pumps in a gram-flow reactor to form a combined solution; adding deionized water with a continuous flow-pump to the combined solution to form a liquid-organic phase solution; extracting the organic phase from the solution; and treating with a solution of t-butyl nitrite with a continuous flow pump in a gram flow reactor to form lomustine.SELECTED DRAWING: None
Owner:PURDUE RES FOUND

Method for co-production of 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride

The invention discloses a method for co-production of 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride, and belongs to the technical field of organic chemical industry, 2, 4-dichlorofluorobenzene is used as a raw material, alkylation and reaction with tert-butyl nitrite are performed to generate oxime, and then hydrochloric acid hydrolysis is performed to generate 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride; according to the method, co-production of the 2, 4-dichloro-5-fluoroacetophenone and the hydroxylamine hydrochloride is innovatively realized, not only are high yield and high purity of the target product 2, 4-dichloro-5-fluoroacetophenone ensured, but also the nitrogen element in the reaction is recycled and converted into the hydroxylamine hydrochloride with high additional value, and the atom economy is remarkably improved; according to the method, the operation process is greatly simplified, the use of dangerous reagents is avoided, and the intrinsic safety and environmental friendliness of the process are improved from the source; the method is simple to operate, safe and environment-friendly, the production cost is effectively reduced, and the market competitiveness of the product is enhanced.
Owner:SHANDONG GUOBANG PHARMA +1

Synthesis method of deuterated methyl selenide compound

PendingCN120987820AOrganic chemistry methodsSandmeyer reactionBenzene
The invention relates to a synthetic method of a deuterated methyl selenide compound, which is characterized in that aromatic amine and deuterated methyl selenyl benzene sulfinate are subjected to Sandmeyer reaction in an organic solvent under the air condition and the action of tert-butyl nitrite to obtain the deuterated methyl selenide compound. The method has the advantages of simple reaction conditions and high product yield and purity, develops a new synthesis route and method for preparation of the deuterated methyl selenide compound, and has good application potential and research value.
Owner:WENZHOU MEDICAL UNIV

Preparation method of visible light induced alpha-germanium oxime compound

The invention belongs to the technical field of organic synthesis, focuses on innovation of a preparation method of an organic germanium compound, and particularly provides a novel photochemical synthesis path of an alpha-germanium oxime compound. According to the method, germane hydride, olefin and tert-butyl nitrite are taken as starting raw materials, and under the condition that no photocatalyst is added, only an ultraviolet light source is utilized for irradiation, so that the germanium-based / oximido-based bifunctionalization reaction of olefin is successfully realized for the first time. The method has the advantages of environmental friendliness, mild conditions, simplicity and convenience in operation, high atom economy, wide substrate application range and the like. The method can be used for modifying the drug molecule derivative after germanium group / oximidation, opens up a way for constructing an organic germanium compound with potential biological activity and pharmacological action, and is expected to play an important role in the field of medicine research and development.
Owner:HENAN INST OF ENG +1

A 3-bromofluorenone and its preparation method

The application provides a kind of 3-bromofluorenone and preparation method thereof, it relates to the technical field of organic photoelectric material.The method is prepared by using 2-bromofluorenone and benzophenone imine under the condition of palladium catalyst to react 2-amino fluorenone, purification is convenient;Using 2-amino fluorenone and N-bromosuccinimide under ice water bath, the impurity can be controlled, purification is convenient, cost is controlled;Using with tert-butyl nitrite can obtain high purity 3-bromofluorenone compound target product;Using N-bromosuccinimide in ice water bath, accurately locate the 3 position of fluorenone, without the help of other catalysts, simplify the reaction;Using the way of dropping tert-butyl nitrite THF solution into the reaction system, can greatly improve the utilization rate of tert-butyl nitrite, finally improve the yield of the whole reaction.The preparation method provided by the application has the advantages of controllable impurity, easy purification and cost economy.
Owner:WEISIPU NEW MATERIAL (SUZHOU) CO LTD

Palladium-catalyzed cyclization extension reaction method of butadienes

The invention relates to a method for a palladium-catalyzed cyclization extension reaction of butadienes. Specifically, under the condition that tert-butyl nitrite is oxidized under the catalysis of palladium, the cyclopentanone compound is obtained through a ring extension reaction of butyl fulvene and water. According to the invention, green and rich water is used as a raw material, and a series of cyclopentanone compounds are obtained under mild conditions.
Owner:DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES

Application of thiazolothiazole fluorescent derivative in sensing detection of butyl nitrite

This invention discloses the application of a thiazo[a]thiazolium fluorescent derivative in the sensing and detection of butyl nitrite. This fluorescent derivative uses the electron-deficient thiazo[a]thiazolium group as the core, with symmetrically connected at both ends a benzene ring with a typical "propeller" conformation and methoxylated triphenylamine at the para- or ortho-position as electron donors, forming a D-A-D type structure. This derivative exhibits high fluorescence quantum yield, excellent intramolecular charge transfer (ICT) characteristics, and good photophysical properties, demonstrating excellent sensing performance for butyl nitrite, including high sensitivity, fast response speed, and short recovery time. Furthermore, this fluorescent derivative is prepared into a fluorescent sensing film with good photochemical stability using a drop-coating method, and then assembled into a device to construct a thin-film fluorescent sensor, demonstrating significant application potential and practical value in the high-sensitivity detection of butyl nitrite.
Owner:SHAANXI NORMAL UNIV

Preparation method of ceftriaxone sodium

PendingCN120574923AFermentationCeftriaxonumMethylating Agent
The invention relates to a preparation method of ceftriaxone sodium, which comprises the following steps: (1) mixing aminothiazole acetic acid, an organic solvent and ethylene glycol, dropwise adding thionyl chloride to carry out primary reaction, concentrating the reaction liquid after the reaction is finished, then adding the organic solvent again and dropwise adding thionyl chloride to carry out secondary reaction to obtain chloroethanol aminothiazole acetate; (2) reacting the chloroethanol aminothiazole acetate with 7-ACT in the presence of immobilized penicillin acylase for synthesis to generate a first intermediate product; (3) reacting the first intermediate product with tert-butyl nitrite under an acidic condition to generate a second intermediate product; (4) reacting the second intermediate product with a methylation reagent under the action of a base catalyst to generate ceftriaxone acid; and (5) reacting the ceftriaxone acid with an inorganic base to generate the ceftriaxone sodium. The preparation method disclosed by the invention is mild in reaction, green and environment-friendly, high in yield and high in purity.
Owner:SUZHOU DAWNRAYS PHARM CO LTD

Preparation method of 4, 6-dichloro-5-methoxypyrimidine

The invention discloses a preparation method of 4, 6-dichloro-5-methoxypyrimidine, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking dimethyl methoxymalonate as a raw material, generating 2-amino-4, 6-dihydroxy-5-methoxypyrimidine from dimethyl methoxymalonate and guanidine salt under the action of sodium ethoxide; then under the action of tert-butyl nitrite, lithium chloride, salicylic acid and tris (pentafluorophenyl) boron, 4, 6-dihydroxy-5-methoxypyrimidine is generated; finally, under the action of phosphorus oxychloride, 4, 6-dichloro-5-methoxypyrimidine is generated. According to the route, in the first step, a 2-aminopyrimidine product is generated through guanidine salt, in the second step, amino is eliminated through azotization, and the synthesis method of the compound is enriched.
Owner:安徽英特美科技有限公司

4-(formoximino)-fluoro-2-quinolinones and a method for their synthesis

This invention discloses a 4-(formaldehyde oxime)-fluoro-2-quinolinone compound and its synthetic method, belonging to the fields of organic synthetic chemistry and medicinal chemistry. Using halogen-containing fluoro-N-(2-vinylphenyl)acetamide compounds as starting materials, this invention utilizes a visible light-induced tandem cyclization reaction to obtain 4-(formaldehyde oxime)-fluoro-2-quinolinone compounds in high yield. This invention employs greener and cleaner visible light as an energy source and uses inexpensive and readily available tert-butyl nitrite and trimethylamine borane as dual-role reagents (hydrogen transfer reagent and oxime source) and halogen atom transfer reagent, respectively, avoiding the use of expensive transition metal catalysts. The raw materials are simple and readily available, the process is environmentally friendly, and the target product yield is high.
Owner:YANTAI UNIV

Visible light-driven deaminative bromosulfonylation method

PendingCN122647381AN-butyl nitriteOrganosolv
The application discloses a visible light driven deaminative bromosulfonylation method. The method comprises the following steps: under the protection of inert gas, sulfonamide shown in formula (I), alkyne shown in formula (II), 10H-phenothiazine and carbon tetrabromide are dissolved in an organic solvent, tert-butyl nitrite and trifluoroacetic acid are added, and reaction is carried out under visible light irradiation to obtain (E)-beta-bromo vinyl sulfone shown in formula (III); wherein, R 1 is selected from aryl, substituted aryl, heteroaryl, alkyl or cycloalkyl; R 2 is selected from aryl, substituted aryl, heteroaryl, alkyl or cycloalkyl; R 3 is selected from alkyl; the photocatalyst is 10H-phenothiazine; the bromine source is carbon tetrabromide; the organic solvent is 1,4-dioxane, N,N-dimethylformamide, dimethyl sulfoxide or acetonitrile; and the wavelength of visible light is 420-520 nm. The method has the advantages of high stereoselectivity, mild reaction condition and wide substrate application range.
Owner:CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY

Method for efficiently preparing fluorene derivative by ball milling method

The invention relates to the technical field of chemistry and chemical engineering, in particular to a method for efficiently preparing fluorene derivatives through a ball milling method. The method comprises the following steps: under the protection of an inert gas atmosphere, carrying out a ball-milling reaction on raw materials including 2-amino-2 '-iodobiphenyl, tert-butyl nitrite, a 1, 3-dicarbonyl derivative, palladium trifluoroacetate and potassium carbonate to obtain the 9, 9-disubstituted fluorene derivative as shown in a formula I. The invention provides a method for efficiently preparing the fluorene derivative through a ball-milling method. The preparation method can solve the technical problem that the preparation method of the organic photoelectric material containing the fluorene unit in the prior art is tedious and complicated in multiple steps, and has the characteristics of simplicity, high efficiency and environmental protection.
Owner:FUQING BRANCH OF FUJIAN NORMAL UNIV

A compound for light-controlled release of nitric oxide, its preparation and application

A compound for light-controlled nitric oxide release, as well as its preparation and application. The compound has a molecular structure of #imgabs0#. The preparation method comprises reacting 4-bromo-N,N-dimethylaniline and 5-aldehyde-2-thiopheneboronic acid under the action of a first base and a first catalyst to generate compound 1; then reacting compound 1 with tert-butyl nitrite under the action of a second catalyst to obtain compound 2; and then reacting compound 2 with (3,5,5-trimethylcyclohex-2-enylidene)malononitrile under the action of a second base to obtain a compound for light-controlled nitric oxide release. The application of the compound for light-controlled nitric oxide release is that the molecule can controllably generate nitric oxide under the stimulation of light, and a quantitative amount of nitric oxide regulates neural differentiation in vivo, thereby promoting neural damage repair. The present invention can accurately and controllably release nitric oxide, realize controllable on-demand release of NO, and can monitor cell differentiation in real time.
Owner:XI AN JIAOTONG UNIV

Synthesis method of deuterated chlorobenzene-D4

The invention belongs to the technical field of preparation of deuterated organic compounds, and particularly relates to a synthetic method of deuterated chlorobenzene-D4, which comprises the following steps: reacting deuterated aniline, benzyltriethylammonium chloride and tert-butyl nitrite to prepare the deuterated chlorobenzene-D4. According to the method, the synthesis process is mild and easy to control, the requirement for equipment is low, the raw materials are low in price and high in utilization rate, and the purity and the deuteration rate of the prepared deuterated chlorobenzene-D4 are high.
Owner:PERRY TECH CO LTD

A synthetic method of fluralaner

The present invention belongs to the technical field of chemical synthesis, and particularly relates to a method for synthesizing flecainide. 4-Bromo-2-methyl-benzoic acid undergoes a substitution reaction with n-butyl vinyl ether to generate 4-acetyl-2-methylbenzoic acid, which successively undergoes a condensation reaction with 2-amino-N-(2,2,2-trifluoroethyl)acetamide, an addition reaction with 3,5-dichlorobenzaldehyde, an isocyclization reaction with tert-butyl nitrite, a substitution reaction with (trifluoromethyl)trimethylsilane, and preferably a heating reaction to generate flecainide. By controlling the types and dosages of catalysts in each step of the reaction, each step of the reaction has a high yield, and finally flecainide is obtained with a high yield.
Owner:HANGZHOU FENGXI BIOTECHNOLOGY CO LTD +1

A functionalized MXene modification method, a diaphragm preparation method and application

The invention discloses a modification method, a diaphragm preparation method and application of functionalized MXene, and belongs to the technical field of liquid flow battery. The modification method comprises: preparing MXene from MAX ceramic powder by mixed acid etching method; preparing MXene nanosheets; adding dried MXene nanosheets, amino-containing aromatic organic small molecules and diazonium salt initiators in a molar ratio of 1-1.5:7-9.5:7-9.5, wherein the diazonium salt initiator is tert-butyl nitrite or isoamyl nitrite; vacuuming, reacting for 8-12 hours, and the temperature is 60-80°C to obtain functionalized MXene covalently grafted with organic small molecules. The invention is based on a mild diazonium salt reaction, and different functional groups can be connected according to application requirements to obtain functionalized MXene covalently grafted with organic small molecules, thereby improving the electrochemical performance of liquid flow battery diaphragm materials.
Owner:CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY

Preparation method of 2, 3, 5, 6-tetrafluorophenyl-1, 4-disulfonyl chloride

The invention discloses a preparation method of 2, 3, 5, 6-tetrafluorophenyl-1, 4-disulfonyl chloride, and belongs to the technical field of organic intermediates. The preparation method comprises the following steps: taking 2, 3, 5, 6-tetrafluorop-phenylenediamine, DABSO and a hydrochloric acid aqueous solution as raw materials, and reacting in acetonitrile in the presence of a catalyst and tert-butyl nitrite to obtain 2, 3, 5, 6-tetrafluorophenyl-1, 4-disulfonyl chloride. In the method, the copper porphyrin catalyst is the key, the catalytic effect is good, and the yield is obviously reduced when the copper porphyrin catalyst is replaced with other copper catalysts. All the raw materials can be conveniently purchased on the market, the target product is synthesized through a one-step method, three wastes are few, the yield is high, and industrial production is easy.
Owner:NINGXIA ZHONGTONG BIOTECHNOLOGY CO LTD

Preparation method of isochromanone compound

The invention discloses a preparation method of an isochromanone compound, and belongs to the technical field of chemical synthesis. The invention provides a preparation method of an isochromanone compound, which comprises the following steps: by taking isochromanone as a raw material, N-hydroxyphthalimide (NHPI) as a catalyst and tert-butyl nitrite (TBN) as an initiator, carrying out oxygen oxidation in a micro-channel reactor in the presence of an organic solvent to obtain isochromanone. According to the preparation method, the reaction conditions are milder while the high yield can be guaranteed, introduction of metal ions and generation of acid waste liquid in the traditional technology are overcome, oxygen is selected as an oxidizing agent, the price is low, the oxidizing agent is easy to obtain, a by-product is water, pollution is avoided, and the method is suitable for industrial production. The microchannel reactor with high heat transfer efficiency and high mass transfer efficiency is used for strengthening the molecular oxygen oxidation reaction process, and a brand new way is provided for solving the problems that the oxidation reaction efficiency is low, the oxidizing agent atom economy is poor, the safety risk is large, and amplification is difficult.
Owner:LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY

A kind of synthetic method of meta-hydroxylamine bitartrate

The invention discloses a synthesis method of meta-hydroxylamine bitartrate: meta-hydroxyphenylacetone is used as a raw material to react with a hydroxyl protecting agent in an organic solvent to form an intermediate compound IV, and then an oximation reaction is carried out with n-butyl nitrite to form a hydroxylamine intermediate, Pd / C catalytic reduction-debenzylation reaction, L-tartaric acid salt separation to obtain a crude L-meta-hydroxylamine bitartrate, and then refined and decolorized with anhydrous ethanol to obtain meta-hydroxylamine bitartrate with a purity of more than 99.6%. The method of the present invention is simple to operate, convenient for post-processing, and high in raw material conversion rate, so that high-purity meta-hydroxylamine bitartrate can be obtained, which is an effective method that is easy to industrialize.
Owner:YUMEN QIANHUA PHARM CO LTD

A 1,5-disubstituted 1,2,3-triazole derivative and a synthesis method thereof

The invention discloses a 1,5-disubstituted 1,2,3-triazole derivative and a synthesis method thereof. A 1,5-disubstituted 1,2,3-triazole derivative synthesis method, using 2,2-difluoro-2-arylethane-1-amine as a raw material, acetic acid as a catalyst, and tert-butyl nitrite as an oxidant, dissolving the 2,2-difluoro-2-arylethane-1-amine in an organic solvent, then adding acetic acid and tert-butyl nitrite to the above solution, and reacting at 25 to 60 ° C to obtain the 1,5-disubstituted 1,2,3-triazole derivative. The present invention can realize the synthesis of 1,5-disubstituted 1,2,3-triazole derivatives without azide as a raw material. The synthesis method has the advantages of high atom economy, high regioselectivity, cheap and easy-to-obtain raw materials, mild reaction conditions, simple and safe operation, etc. The synthesized 1,5-disubstituted 1,2,3-triazole derivatives are widely present in natural products and drug molecules, have good biological activity, and are important pharmaceutical intermediates.
Owner:PINGDINGSHAN UNIVERSITY

Process for the preparation of sulfonic acid derivatives by sulfonamide deamination

The application discloses a method for synthesizing sulfonic acid derivatives, which comprises the following steps: mode one, first, sulfonamide compounds, tert-butyl nitrite, a chlorine source and a catalyst are subjected to a diazotization chlorination reaction in an organic solvent under nitrogen condition, or a nucleophile is additionally added for reaction, so that sulfonic acid derivatives are obtained; mode two, a two-step method is adopted, first, sulfonamide compounds, tert-butyl nitrite and a catalyst are subjected to a diazotization reaction in an organic solvent under nitrogen condition, and then a nucleophile is added for reaction, so that sulfonic acid derivatives are obtained. The method has the advantages of simple steps, low cost and simple operation, can overcome the shortcomings of high pre-functionalization of substrates, easy moisture absorption of reactants, metal catalysis of reaction and complicated steps in the prior art, and can play an important role in the research field of sulfonamide conversion and application.
Owner:CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY

A preparation method of Michler's ketone derivative

The present invention provides a method for preparing a Michler's ketone derivative, which belongs to the field of organic synthesis. A method for preparing a Michler's ketone derivative comprises the following steps: mixing bis(4-(dialkylamino)phenyl)methane, a catalyst, a 1-alkyl-3-methylimidazolium hydrogen sulfate ionic liquid, oxygen and water for an oxidation reaction to obtain the Michler's ketone derivative; the catalyst comprises 2,3,5,6-tetrachlorobenzoquinone and tert-butyl nitrite; the Michler's ketone derivative comprises the structural formula shown in Formula I; and R1 and R2 are independently C2 to C18 alkyl groups. The 1-alkyl-3-methylimidazolium hydrogen sulfate ionic liquid can promote the decomposition of tert-butyl nitrite into nitrogen oxides required for the oxidation reaction, thereby improving the selectivity and yield of the Michler's ketone derivative. At the same time, the use of the catalyst of the present invention to catalyze the oxidation reaction avoids the use of a transition metal catalyst and does not have the problem of metal residue; oxygen is used as an oxidant, which is environmentally friendly.
Owner:HANGZHOU TOKA INK CO LTD

A method for one-pot synthesis of an oxime ether fungicide intermediate

The application relates to a one-pot method for synthesizing an intermediate oxime ether of a bactericide, and belongs to the technical field of organic synthesis. The method flow comprises the following steps: Step 1: adding o-halotoluene, methyl glyoxylate, methoxyamine hydrochloride and a solvent into a reaction bottle, wherein X in the o-halotoluene is chlorine, adding a base and a catalyst, the catalyst is Cu-TMEDA, and the reaction is carried out after heat preservation; Step 2: after the reaction is completed, water is added for washing, and the organic phase is concentrated under reduced pressure to recover the solvent to obtain the oxime ether. In the application, compared with a traditional oxime ether synthesis method, the oxime ether is synthesized by using o-halotoluene, methyl glyoxylate and methoxyamine hydrochloride as raw materials in a one-pot catalytic synthesis mode, the reaction process is safe and reliable, the raw material cost is low, and the three-waste output is less. The oxime ether synthesis method is simple and efficient, the reaction condition is mild, a toxic sodium cyanide reagent or flammable and explosive tert-butyl nitrite is not needed, the reaction process is safer, and the method is suitable for industrialized scale production.
Owner:LIAONING ZHONGHUI BIOTECHNOLOGY CO LTD